CN101171368A - Vaporizer and method of vaporizing a liquid for thin film delivery - Google Patents

Vaporizer and method of vaporizing a liquid for thin film delivery Download PDF

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Publication number
CN101171368A
CN101171368A CNA2006800157285A CN200680015728A CN101171368A CN 101171368 A CN101171368 A CN 101171368A CN A2006800157285 A CNA2006800157285 A CN A2006800157285A CN 200680015728 A CN200680015728 A CN 200680015728A CN 101171368 A CN101171368 A CN 101171368A
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liquid
vaporizer
pressure
gas
valve
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Chinese (zh)
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P·梅内吉尼
A·沙吉
D·史密斯
W·克拉克
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MKS Instruments Inc
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MKS Instruments Inc
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
    • C23C16/4485—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by evaporation without using carrier gas in contact with the source material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01B—BOILING; BOILING APPARATUS ; EVAPORATION; EVAPORATION APPARATUS
    • B01B1/00—Boiling; Boiling apparatus for physical or chemical purposes ; Evaporation in general
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Vapour Deposition (AREA)
  • Filling Or Discharging Of Gas Storage Vessels (AREA)

Abstract

A vaporizer including an inlet for liquid and an outlet for gas, a gas valve controlling gas flow to the outlet of the vaporizer, and means for heating liquid flowing between the liquid inlet and the gas valve. The vaporizer also includes means for increasing a heat transfer rate of the liquid flowing between the liquid inlet and the gas valve, and for causing a pressure drop in the liquid so that a pressure of the liquid drops below a vapor transition pressure of the liquid upon reaching the gas valve. The pressure drop occurs under isothermal conditions, and the liquid is vaporized on demand only when the valve is opened. The means for increasing a heat transfer rate and for causing a pressure drop can be a plug of porous media.

Description

Film forming vaporizer of vaporised liquid and method
Technical field
The present invention relates generally to evaporation film forming vaporizer of precursor gases and method.
Background technology
It is very complicated to make or produce semiconducter device, usually needs, and for example, synchronously careful and accurate measurement ground will reach 12 kinds of gas delivery in Processing Room.In manufacturing process, use different prescriptions, and semiconducter device needs a lot of discrete treatment steps, for example clean, polishing, oxidation, mask, etching, doping and metallization.Used step and order thereof and related material all influence the manufacturing of certain device.
Along with device size continues to be reduced to below the 90nm, the semi-conductor developing direction is pointed out, a lot of application need alds or ALD technology, and for example deposition is used for the blocking layer of copper-connection, and forms the tungsten nucleating layer.In ALD technology, the crystal column surface of flowing through in the Processing Room of two or more precursor gases (precursor gas) under being maintained at vacuum.Two or more precursor gases in an alternating manner or pulse mode flow, the position of gas and crystal column surface or functional group are reacted.When all available sites were saturated by a kind of precursor gases (for example, gas A), reaction stopped and using rinsing gas that unnecessary precursor molecule is removed from Processing Room.When next precursor gases (that is gas B) repeats said process when flowing through crystal column surface.Circular in definition is precursor A pulse, flushing, precursor B pulse, flushing.Repeat this order up to reaching final thickness.These sequentially realize each cyclic deposition unitary film from the limiting surface reaction.
The pulse that precursor gases enters Processing Room utilizes the control of on/off-type gas trap usually, and wherein gas trap is opened predetermined period of time simply, keeps container transport to Processing Room from heating the precursor gases of pre-determined quantity.In addition, also can the using gas mass flow controller in short time interval, carry and to repeat gas flow, the self-contained system that this gas mass flow amount controller is made up of transmitter, gas control valve and control and signal treatment circuit.
Under many circumstances, precursor gases forms by vaporised liquid and solid.The standard technique of vaporised liquid is to use liquid mass flow director and independent evaporator unit at present, and perhaps Zu He liquid mass flow director and vaporizer is transported to heating with the precursor gases with evaporation and keeps container.This liquid is at first measured from source container by the liquid mass flow director, then by the evaporator unit evaporation, is transported to heating then and keeps container.Then, use on/off-type gas trap or gas mass flow amount controller to keep container transport to Processing Room from heating the precursor gases of desired number.But the shortcoming of this technology is the cost height.Liquid mass flow director and evaporator unit also spend a large amount of expenditures.In addition, a lot of ALD precursors have quite high demand for heat, and owing to condensation is difficult to carry out exactly flow control, and be easy to decompose in undesirable mode before use.
The ALD precursor can be according to purposes and great changes have taken place.New precursor is still at development﹠ testing, so that satisfy different matrix and deposit film demand.Three kinds of precursors very commonly used are Al (CH 3) 3(Al 2O 3Deposit film), HfCl 4(HfO 2Deposit film) and ZrCl 4(ZrO 2Deposit film).The oxygen precursor of every kind of these gases is H normally 2O or O 2Or O 3Utilize ALD or CVD technology to comprise Ni, W, SiO by sedimentary other film type 2, Ta 2O 5, TaN, TiO 2, WN, ZnO, ZrO 2, WCN, Ru, Ir, Pt, RuTiN, Ti, Mo, ZnS, WN xC y, HfSiO, La xCa yMnO 3, CuInS 2, In 2S 3, HfN, TiN, Cu, V 2O 5, and SiN.But, should be noted that the present invention is not limited to be applied to any particular precursor or technology.
Still demand evaporate precursor material film forming new and improved vaporizer and method in addition, for example in ald (ALD) technology.Preferably, new and the improved vaporizer and the method for evaporation precursor gases are compared with the existing method and apparatus of evaporation precursor material, and its design is quite simple and relatively more cheap.In addition, preferably, new and improved vaporizer that is used to evaporate and method provide steam as required when the actual metered steam, this with use before form steam and store steam different.
Summary of the invention
The invention provides a kind of vaporizer, comprise the outlet of the inlet that receives liquid and output gas, pilot-gas flows to the gas trap of evaporator outlet, and heating unit that will flowing fluid heating between liquid inlet and gas trap.Described vaporizer also comprises the heat transfer rate increase of flowing fluid between liquid inlet and the gas trap and makes the device that flowing fluid generation pressure falls between liquid inlet and the gas trap, thereby the pressure of liquid after arriving gas trap drops to below the steam pressure phase transition of liquid.
According to one aspect of the invention, cause that pressure between fluid intake and the gas trap falls and the device that increases the heat transfer rate of flowing fluid between fluid intake and the gas trap comprises the porous plug that connects fluid intake and gas trap.
According to a further aspect of the present invention, vaporizer is combined in the system with the precursor gases of pulsed mass flow input semiconductor processing chambers, the actual measurement of wherein said system flow into the material quantity (quality) of Processing Room and delivery head repeatably with the gaseous substance of exact quantity.
In others and advantage, the invention provides a kind of new and improved vaporizer, and the film forming method of a kind of evaporation precursor gases, for example ald (ALD) technology and other chemical vapor deposition (CVD) technology.This new method with improved vaporizer and evaporation precursor gases is relative in design simple and relatively cheap.In addition, this new and improved vaporizer evaporate liquid (, only when gas trap is opened) when metering as required.
From following detailed description, for persons skilled in the art, it is quite obvious that other aspects and advantages of the present invention will become, and the illustrative examples of the present invention that wherein illustrates and illustrate only is indicative.As understandable, the present invention that can have other with different embodiment, its several details can be made amendment aspect obvious a plurality of, all these does not depart from the present invention.Therefore, accompanying drawing and explanation should think that it is indicative in essence, rather than restrictive.
Description of drawings
Below with reference to the accompanying drawings, the part that wherein has same reference numerals is represented identical parts in institute's drawings attached.In the accompanying drawings:
Fig. 1 has schematically shown the illustrative examples of the vaporizer that constitutes according to the present invention;
Fig. 2 has schematically shown the illustrative examples of the atomic layer deposition system of the vaporizer that comprises Fig. 1;
Fig. 3 has schematically shown the illustrative examples of the pulsed mass flow delivery system of the vaporizer that comprises Fig. 1;
Fig. 4 is the schema of the illustrative examples of expression transport pulse mass rate method, and wherein this method can be used for the pulsed mass flow delivery system of control diagram 3;
Fig. 5 is the side-view of the illustrative examples of the vaporizer of formation according to the present invention;
Fig. 6 is the end view of the vaporizer of Fig. 5;
Fig. 7 is the sectional view of the vaporizer 7-7 along the line of Fig. 5;
Fig. 8 is the sectional view of the vaporizer 8-8 along the line of Fig. 6;
Fig. 9 is the amplification view of a part of the vaporizer of Fig. 5, wherein shows inlet that flows through vaporizer and the liquid that flows into porous plug, and shows the gas that flows out porous plug through the valve module and the outlet of vaporizer; And
Figure 10 flows through the pressure of water of the different porous plug assembly of 4 pore dimensions and the relation curve of porous plug length.
Embodiment
At first with reference to Fig. 1 and 2, the invention provides a kind of new and improved vaporizer 10, and the film forming method of a kind of evaporation precursor gases, for example ald (ALD) technology and other chemical vapor deposition (CVD) technology.In others and advantage, new relative in design simple according to evaporation precursor gases of the present invention with improved vaporizer and method, and relatively cheap.
As illustrated in fig. 1 and 2, vaporizer 10 comprises that the inlet 12 that is used for liquid, the outlet 14 that is used for gas and pilot-gas flow to the gas trap 16 of outlet 14.Vaporizer 10 also comprises the device 18 that causes that steady pressure falls and increases the heat transfer rate of fluxion between liquid inlet and the gas trap between liquid inlet 12 and the gas trap 16.Vaporizer 10 also comprises the device 20 of flowing fluid between heating liquid inlet 12 and the gas trap 16, thereby is reduced to vapor line maintenance homo(io)thermism or rising when following at pressure.Pressure-drop designs 18 enough descends the liquid pressure that enters the liquid inlet fully and apace, the pressure of liquid is dropped to below the steam pressure phase transition (vapor transition pressure), and be evaporated after arriving gas trap.Though not shown, vaporizer 10 also can comprise the transmitter of the temperature of monitoring pressure falling unit 18, and the controller circuitry of controlling heating unit 20 according to temperature.
Vapor pressure is the pressure (if steam mixes other gas, then being dividing potential drop) of steam.In any given temperature,, there is steam and its liquid or solid form equilibrated pressure of this material for predetermined substance.Here it is the saturated vapor pressure of this material under this temperature.The term vapor pressure is often understood to mean saturated vapor pressure.When the pressure of any liquid equals its saturated vapor pressure, the liquid portion evaporation; Liquid and steam reach balance.Suppose temperature-resistantly, if pressure reduces, balance changes towards material gas phase direction, the final all evaporations of liquid.
According to an illustrative examples of the present invention, cause that pressure falls and the device that increases heat transfer rate comprises porous medium plug 18.Be important to note that the pressure of valve outlet port must be lower than the vapor pressure of liquid.Otherwise liquid will flow out porous medium, and gas trap can not cut out.Higher heat transfer rate is to guarantee that steady temperature is essential, because vaporised liquid produces hear rate.If the local temperature of porous medium plug 18 descends, then local saturated vapor pressure descends thereupon, is lower than the pressure in exit sometimes.Then, in porous medium plug 18, will not have any evaporation.
The porous medium that is fit to can from, for example, CT, the Mott company of Farmington (http://www.mottcorp.com) obtains.According to an illustrative examples, porous medium is made by sintering metal.Sintering metal can be made less than 20 microns metal-powder by the mean particle size of presintering.According to another embodiment, the mean particle size of sintered powder is less than 10 microns, and the density of sintering metal is at least 5g/cc.The metal that is used for making plug 18 is selected from following group: stainless steel, nickel and nickelalloy and titanium, but be not limited thereto, so that satisfy particular requirement, for example higher temperature and solidity to corrosion.Particularly, metal and alloy include, but are not limited to: stainless steel 316L, 304L, 310,347 and 430, and Hastelloy C-276, C-22, X, N, B and B2, Inconel 600,625 and 690, Nickel 200 and Monel 400 (70Ni-30Cu), titanium, and alloy 20.
According to another illustrative examples of the present invention, porous medium plug 18 is made by stainless steel 316L, and is suitable at pressure 30psig (with the metering pressure of normal atmosphere as 0 benchmark) with 10sccm (standard cubic centimeter of per minute) flow velocity the supply of nitrogen.According to another illustrative examples, porous medium plug 18 is made by stainless steel 316L, and is suitable at 30psig with 50sccm flow velocity supply N 2316L makes by stainless steel, and is suitable at 30psig with 250sccm flow velocity supply N 2Perhaps make, and be suitable at 30psig with 50sccm flow velocity supply N by Nickel200 2According to an illustrative examples of the present invention, porous medium plug 18 is cylindrical and longilineal, can comprise single elongated porous medium spare, perhaps can comprise independent inserts, and they are deposited in and form elongated porous medium assembly together.
Porous medium plug 18 also can be assembled into by the interior cylinder that coaxially is received in the overcoat, and interior cylinder can comprise different porous mediums with overcoat.This assembly will provide the steam of parallel-flow.
The porosity of porous medium plug 18 or pore dimension control pressure fall.According to an illustrative examples, porous medium plug 18 comprises the inserts of single-piece, is made into by sintering two different size imitation frosted glass into the single-piece goods.Every kind of imitation frosted glass size will be corresponding to different aperture size or porosity.
Porous medium plug 18 can comprise the material beyond the metal, and for example quartzy, pottery (sapphire, aluminum oxide, aluminium nitride etc.), and polymeric material comprise Teflon, PFA, PTFA etc.
Cause that pressure falls and the device 18 that increases heat transfer rate can have other form alternatively, for example, but be not limited to: long, thin, broad wool tubule, long, thin, spiral capillary, a branch of fine, soft fur tubule, or laminar flow element.
As shown in Figure 2, the vaporizer 10 of Fig. 1 can be used to Processing Room 60 that the vaporized gas precursor is provided so that form film, for example in ald (ALD) technology or other chemical vapor deposition (CVD) technology.An illustrative examples that comprises the atomic layer deposition system 11 of vaporizer 10 shown in Figure 1 is illustrated among Fig. 2, and comprises liquid precursor source 30, conveying chamber 40 and the gas trap 50 that conveying chamber 40 is connected to Processing Room 60.As shown in the figure, the inlet 12 of vaporizer 10 is connected to fluid supply 30, and the outlet 14 of vaporizer is connected to conveying chamber 40.Vaporizer 10 is used to evaporate from the Liquid precursor of fluid supply 30 and with evaporated liquid, and perhaps precursor gases is transported to conveying chamber 40.Though not shown, conveying chamber 40 also can heat.Then, open and close gas trap 50,, in Processing Room, form film as required so that precursor gases is transported to Processing Room 60 from conveying chamber 40.
Referring to Fig. 3, represent an illustrative examples of the mass flow delivery system 100 of formation, and comprise the vaporizer 10 of Fig. 1 according to the present invention.Fig. 4 shows an illustrative examples of the method 200 of carrying mass rate, and wherein this method is used for the pulsed mass flow delivery system of application drawing 3.System 100 and method 200 are used in particular for processing gas free of contamination, the quantity accurate measurement is transported to semiconductor processing chambers, for example the Processing Room of ALD or CVD device.In fact mass flow delivery system 100 and method 200 measure the material quantity (quality) that flows into Processing Room.In addition, system 100 and method 200 provide highly repeatably the gaseous substance with exact quantity, so that be applied to semiconductor fabrication process, and for example ALD or CVD technology.
Referring to Fig. 3, mass flow delivery system 100 comprises the maintenance space 140 that is connected to vaporizer 10, and the valve 150 of the mass rate that keeps space 140 is flowed out in control.Illustrative examples according to the present invention, valve 150 comprises the on/off-type valve with about 1 to 5 millisecond of time of response that is exceedingly fast.Mass flow delivery system 100 also has pressure transmitter 104, so that measure the pressure that keeps in the space 140, and temperature sensor 106, be used to measure on the maintenance space 140 or the temperature in the maintenance space 140.Pressure transmitter 104 also has about 1 to 5 millisecond quickish time of response.According to an illustrative examples of the present invention, temperature sensor 106 contacts keep the wall in space 140, and the temperature survey to it is provided.The example that is fit to be applied to the pressure transmitter 104 of delivery system 100 of the present invention comprises the Baratron that can buy from the present patent application people The board pressure transmitter, MA, the MKS Instruments company (http://www.mksinst.com) of Wilmington.The valve 150 that is fit to is, for example, is used for the diaphragm valve of ald, can be from Ohio, and the Swagelok company of Solon obtains (www.swagelok.com).
The input/output device 108 of mass flow delivery system 100 receives required mass rate (directly from the operator, perhaps indirectly by wafer processing computer control unit), and computer control unit (that is, computer processing unit or " CPU ") 102 is connected to pressure transmitter 104, temperature sensor 106, outlet valve 150 and input/output device 108.Input/output device 108 also can be used to import other processing instruction, and the quality that can be used to provide system 100 to carry is indicated (directly outputing to the operator, perhaps indirectly by wafer processing computer control unit).For example, input/output device 108 can comprise the Personal Computer with keyboard, mouse and watch-dog.
According to an illustrative examples of the present invention, the method 200 of controller 102 execution graphs 4 of the mass flow delivery system 100 of Fig. 3.Referring to Fig. 3 and 4, controller 102 is programmed receiving required mass rate (that is, setting point) by input/output device 108, as Fig. 4 202 shown in, close outlet valve 150, as Fig. 4 204 shown in, open the valve 16 of vaporizer 10, as Fig. 4 206 shown in, applying pressure transmitter 104 is measured the pressure that keeps in the space 140, as Fig. 4 208 shown in, and the pressure in keeping space 140 closes inlet valve 16 when reaching predeterminated level, as Fig. 4 210 shown in.The pressure of predeterminated level is user-defined, and can provide by input/output device 108.For example, the pressure of predeterminated level can comprise 200torr.
At scheduled wait after the time, keep this moment the gases in the space 140 can reach equilibrium state, open outlet valve 150, discharge a certain amount of gas from keeping space 140, as Fig. 4 212 shown in.The scheduled wait time is user-defined, can provide by output/take-off equipment 108.For example, the scheduled wait time can comprise 3 seconds.When the amount of expellant gas equals user-defined required mass rate, close outlet valve 150, as Fig. 4 214 shown in.Outlet valve 150 is opened only very short time (for example, 100 to 500 milliseconds).Controller 102 is provided to input/output device 108 with the amount of expellant gas then.
Other operating method also is fine.For example, in some cases, can wish to keep space 140 to be filled into setting pressure, thereby before filling the maintenance space once more, can carry the gas that keeps the multiple doses in the space by outlet valve.In other cases, can in one period cycle for a long time, carry a certain amount of gas, wherein open outlet valve (for example, 0.5 to 30 second) for a long time.In addition, by using a plurality of valves can prolong the work-ing life of valve at inlet or outlet.At a time only there is one to be pulse manipulated in two valves, and when first defective valve, can uses second valve.In order in opening or closing pattern, to allow defective valve, just need 4 valves: two series connection, these two pairs of parallel connections.The U.S. Patent application No.11/015465 that on December 17th, 2004 submitted to, its title is for " Pulsed Mass Flow Deliver System and Method " and transfer applicant of the present invention, disclosed this structure, and this patent publication us is in full in conjunction with being hereby incorporated by reference.
To high-voltage applications, the gas temperature in the maintenance space 140 of system 100 can use temperature probe (temperature probe) 106 to detect.But for low pressure applications and fast temperature transition, using the probe measurement temperature may not be enough fast for accurate reading.Under the situation of low pressure applications and fast temperature transition, use the real-time physical model of estimating gas temperature, this will be described below.
For some precursor materials, simply by being heated enough vapor pressures that may be difficult to realize material.For example, some materials can excessive decomposition reach the enough vapor pressures that are used to carry when heating, reduce the efficient of deposition process.In other cases, may enough evaporate required temperature does not wish so high.In these cases, precursor material can be dissolved in the appropriate solvent, then evaporation.The example of solvent comprises various alcohol, ether, acetone and oil.Can suitably use the organic or inorganic solvent according to specific application.Supercritical CO 2 can be used as the active solvent of various materials.
According to perfect gas law, keep the total mass m in the space 140 to be
m＝ρV＝(P/RT)V (1)
In the formula, ρ is a density, and V is a volume, and P is an absolute pressure, and T is an absolute temperature, and R is a gas law constant.
Density dynamic change in keeping space 140 is:
dρ/dt＝-(Q outρ STP/V) (2)
In the formula, Q OutBe from keeping space 140 effusive flows, ρ STPIt is the gas density under standard temperature and pressure (STP) (STP) condition.
Keep the temperature dynamic in the space 140 to be changed to:
dT/dt＝(ρ STP/ρV)Q out(γ-1)T+(Nuκ/l)(A w/VC vρ)(T w-T) (3)
In the formula, γ is the ratio of specific heat, and Nu is the Nusslets number, and κ is the thermal conductivity of gas, C vBe constant volume specific heat, l is the characteristic length of conveying chamber, and Tw is the wall temperature in the maintenance space 140 that provides of temperature probe 106.
Rate of discharge Q OutCan estimate by following formula:
Q out＝-(V/ ρSTP)[(1/RT)(dρ/dt)-(P/RT 2)(dT/dt)] (4)
In order to calculate from keeping the total mass Δ m of space 140 outputs, the Q of formula (4) substitution formula (3) OutCalculate to keep in the space 140 time=gas temperature T (t) during t, relative with use temperature probe 106 among Fig. 3.Pressure transmitter 104 provide keep in the space 140 time=pressure P (t) during t.
At time t 0With time t *Between from the total mass Δ m that keeps space 140 outputs be:
Δm＝m(t 0)-m(t *)＝V/R[(P(t 0)/T(t 0))-(P(t *)/T(t *))] (5)
In others and advantage, mass flow delivery system of the present invention and method, for example Fig. 3 and 4 illustrative examples, actual measurement flows into the amount of the material (quality) of Processing Room.In addition, system and method provides the gaseous substance that highly can repeat with exact quantity, is applied to semiconductor fabrication process, for example ald (ALD) technology.
Fig. 5 to 9 shows another illustrative examples of the vaporizer 300 that constitutes according to the present invention, and wherein vaporizer 300 comprises the valve body 350 that contains porous plug assembly 318.Vaporizer 300 is similar to the vaporizer 10 of Fig. 1, thereby identical part is added " 3 " expression with the same reference numerals front.
The vaporizer 300 of Fig. 5 to 9 utilizes diaphragm valve 316 to carry out ald.Be suitable for the diaphragm valve 316 of ald, comprise valve body 350, for example, can be from Ohio, the Swagelok company of Solon obtains (www.swagelok.com).
In the illustrative examples shown in Fig. 5 to 9, valve body 350 comprises the female connector of inlet 312 and outlet 314.Represent better that as Fig. 7 to 9 valve body 350 limits valve seats 352, from 312 access roades 354 that extend to valve seat 352 that enter the mouth, and the exit passageway 356 that extends to outlet 314 from valve seat 352.Represent better that as Fig. 7 valve body 350 also limits the hole 360 that receives well heater 320.Represent better that as Fig. 8 to 9 valve body 350 also defines the hole 370 that receives temperature monitor 321.
Porous plug assembly 318 is positioned at the access road 354 of valve body 350.In illustrated illustrative examples, porous plug assembly 318 is cylindrical and elongated, and comprises the single elongated porous medium spare that is received in the solid metal sleeve.Alternatively, the porous plug assembly can comprise independent inserts, and they are deposited in and form elongated member together, and inserts can comprise different porous medium (that is, providing different in flow rate at different pressures).
The relation curve of Figure 10 pressure that is imaginary liquid when steady temperature is flowed through four porous plug assemblies of different aperture size K1 and K2 and porous plug length.In illustrative example, the length overall of assembly is about 0.014m, and assembly also has the first part that pore dimension is K1, and pore dimension is the second section of K2.A porous plug assembly comprises K1=K2=2.8e-13m 2Another assembly comprises K1=5.6e-14m 2And K2=5.5e-13m 2Additional assembly comprises K1=3.0e-14m 2And K2=2.8e-12m 2Another assembly comprises K1=5.6e-14m 2And K2=1.4e-12m 2Curve table illustrates, and each porous plug assembly evaporated liquid before the assembly of flowing through.
The illustrative examples of describing in this specification sheets provides as signal, and it is not restrictive, persons skilled in the art are not breaking away from the present invention in its broad aspect and under the situation of the spirit or scope that provide in as claims, can make different remodeling, combination and alternative.

Claims (26)

1. vaporizer comprises:
The liquid inlet;
Pneumatic outlet;
Pilot-gas flows to the gas trap of pneumatic outlet;
Will be between liquid inlet and gas trap the heating unit of flowing fluid heating; And
The device that makes flowing fluid between liquid inlet and the gas trap produce that pressure falls and the heat transfer rate of flowing fluid between liquid inlet and the gas trap is increased, thus when arriving gas trap, the pressure of liquid drops to below the steam pressure phase transition of liquid.
2. vaporizer according to claim 1 is characterized in that, describedly is used to produce that pressure falls and the device that increases heat transfer rate comprises the porous medium plug.
3. vaporizer according to claim 2 is characterized in that porous medium comprises sintering metal.
4. vaporizer according to claim 3 is characterized in that, sintering metal is to be made less than 20 microns metal powder by the presintering mean particle size.
5. vaporizer according to claim 4 is characterized in that the mean particle size of sintered part is less than 10 microns.
6. vaporizer according to claim 3 is characterized in that, the density of sintering metal is 5g/cc at least.
7. vaporizer according to claim 3 is characterized in that, described metal is selected from: stainless steel, nickel and nickelalloy and titanium.
8. vaporizer according to claim 3 is characterized in that, the porous medium plug comprises first part with first pore dimension and the second section with second pore dimension, and wherein first part and second section are placed in-line.
9. vaporizer according to claim 3 is characterized in that, the porous medium plug is cylindrical and elongated, and comprises single elongated porous medium spare.
10. vaporizer according to claim 3 is characterized in that the porous medium plug comprises independent inserts, and they are deposited in the elongated member that forms porous medium together.
11. vaporizer according to claim 3 is characterized in that, the porous medium plug is cylindrical and elongated, and comprises the interior cylinder that coaxially is received in the overcoat, and interior cylinder comprises different porous mediums with overcoat.
12. vaporizer according to claim 3 is characterized in that, described valve comprises valve body, and described valve body comprises valve seat, the access road from the entrance extension of vaporizer to valve seat, and the exit passageway that extends to evaporator outlet from valve seat; And described porous medium plug is arranged in described access road.
13. vaporizer according to claim 1 is characterized in that, described heating unit comprises the electrically heated coil, and described vaporizer also comprises temperature sensor.
14. vaporizer according to claim 1 is characterized in that, described valve comprises diaphragm valve.
15. an atomic layer deposition system that comprises vaporizer according to claim 1, and described system also comprises:
Keep the space, wherein the inlet of vaporizer is suitable for being connected to the source of Liquid precursor, and the outlet of vaporizer is connected to the maintenance space; And
Gas trap is used for the maintenance space is connected to Processing Room.
16. system according to claim 15 is characterized in that, also comprises by gas trap being connected to maintenance spatial Processing Room.
17. one kind comprises system vaporizer according to claim 1, that be used to carry required mass gas, and described system also comprises:
Be connected to the maintenance space of evaporator outlet;
Pilot-gas flows out and keeps the spatial outlet valve;
Measure the pressure transmitter that keeps the pressure in the space;
The input unit of the required mass gas of carrying from system is provided;
Controller, described controller is connected to valve, pressure transmitter and input unit, and is programmed the execution following steps:
Receive the gas of required quality via input unit;
Close outlet valve;
Open the valve of vaporizer;
Receive keeping the spatial pressure measuring value from pressure transmitter;
When reaching preset value, the pressure in keeping the space closes the valve of vaporizer;
Wait for the predetermined waiting time, make the gas that keeps in the space reach equilibrium state;
At time=t 0Open outlet valve; And
When the quality of expellant gas equals required quality at time=t *Close outlet valve.
18. system according to claim 17 is characterized in that, the scheduled wait time comprises 3 seconds.
19. system according to claim 17 is characterized in that, t *=100 to 500 milliseconds.
20. system according to claim 17 is characterized in that, t *=0.5 to 30 second.
21. system according to claim 17 is characterized in that, keeps the pressure preset value in the space to allow before the maintenance space requirement refills, and will keep the gas volume of pre-determined quantity in the space to carry through outlet valve.
22. system according to claim 17 is characterized in that, liquid was dissolved in before being transported to evaporator inlet in the suitable solvent.
23. system according to claim 17 is characterized in that, also comprises through outlet valve being connected to maintenance spatial Processing Room.
24. the method for a vaporised liquid comprises:
Receive liquid by inlet;
Gas trap is connected to inlet;
Will be between liquid inlet and gas trap the flowing fluid heating so that even when liquid pressure descends, prevent the temperature decline of liquid;
Increase the heat transfer rate of flowing fluid between liquid inlet and the gas trap; And
Make between liquid inlet and the gas trap flowing fluid produce pressure and fall, thereby when reaching gas trap, the pressure of liquid drops to below the steam pressure phase transition of liquid.
25. method according to claim 24 is characterized in that, uses the porous medium plug that flowing fluid between liquid inlet and the gas trap is produced pressure and falls, and increase the heat transfer rate of liquid.
26. method according to claim 24 is characterized in that, liquid was dissolved in the suitable solvent before being received through inlet.
CNA2006800157285A 2005-03-18 2006-03-03 Vaporizer and method of vaporizing a liquid for thin film delivery Pending CN101171368A (en)

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GB2438807A (en) 2007-12-05
GB0719261D0 (en) 2007-11-14
WO2006101697A2 (en) 2006-09-28
WO2006101697A3 (en) 2007-01-25
KR20070118128A (en) 2007-12-13
TW200706686A (en) 2007-02-16
US20060207503A1 (en) 2006-09-21
JP2008536006A (en) 2008-09-04

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